CN1288732A

CN1288732A - Soft concentrated fish oil capsule and its supercritical CO2 extraction and rectification process

Info

Publication number: CN1288732A
Application number: CN 00109893
Authority: CN
Inventors: 陈受斯; 刘玉; 刘明彦; 欧阳中林
Original assignee: Individual
Current assignee: Individual
Priority date: 2000-07-12
Filing date: 2000-07-12
Publication date: 2001-03-28
Anticipated expiration: 2020-07-12
Also published as: CN1109549C

Abstract

The present invention relates to a high-concentration fish oil soft gel pill and its supercritical CO2 extraction and rectification preparation method. the DHA and EPA contents in described soft gel pill fish oil are 71-74%. DHA/EPA=3-5, and the method of the described supercritical CO2 extraction and rectification includes the processes of extraction, rectifying, separation, receiving and CO2 circulation. Said invented product is high in concentration and DHA/EPA ratio, and good in effect.

Description

Soft concentrated fish oil capsule and supercritical CO thereof 2The method for making of extracting rectifying

The invention belongs to a kind of functional health care product that obtains from natural active matter and preparation method thereof, be specifically related to a kind of soft concentrated fish oil capsule and CO thereof ₂The method for making of super critical extracting and rectifying.

The main component of fish oil is DHA (docosahexenoic acid) and EPA (eicosatetraenoic acid), be human body must but can not self synthetic polyene unsaturated fatty acid, must from food or health product, absorb.Proved already that DHA was in that to improve aspect effects such as intelligence, brain-strengthening, slow down aging remarkable, EPA and DHA synergy can blood fat reducing, cholesterol reducing, antithrombotic, anti-diabetic etc.Reach good result, different crowd is different with the EPA proportion requirement to DHA, take in than being about 5: 1 as gravid woman, infant are best, middle-aged and elderly people then is about 3: 1, and present commercially available fish oil, not only the total content of DHA and EPA is low, and the ratio of the two is taken in ratio far below the best, the ratio of DHA/EPA in the fish oil is improved, and is the key that improves its health-care effect.With solvent extraction, molecularly distilled or general supercritical CO ₂Extraction can only obtain forming complicated mixing extract, can not reach people to DHA and the best requirement of taking in ratio of EPA, seeks a kind of supercritical CO with refining and purification function ₂Extracting process is subjected to people's common concern.

The objective of the invention is to develop a kind of DHA and EPA total content height, the efficient fish oil soft capsule and the supercritical CO thereof of ratio height and adjustable ratio ₂The preparation method of extraction.

The total content of DHA and EPA is 71-74% in the efficient soft concentrated fish oil capsule of the present invention, and its ratio is (3-5): 1, and adopt current techique to make soft capsule.

Supercritical CO of the present invention ₂Extracting process comprises the super critical extraction of raw material, the reception and the CO of separation, products of separated ₂Each unit operations of the circulation of extractant is characterized in that described raw material is rough fish oil ethyl ester, has set up extract at supercritical CO between described extraction and separation unit operation ₂Rectification separative element under the state.

Described supercritical CO ₂The temperature of extraction cells is 34-38 ℃, and pressure changes between 11-14MPa, and extractor is a slack tank, is extracted raw material and puts in advance, can carry out intermittence or continued operation.

Described rectification separative element is divided into four sections, and 1 section temperature is 37-39 ℃, and 2 sections is 42-44 ℃, and 3 sections is 47-49 ℃, and 4 sections is 52-54 ℃, and the pressure of whole rectifying column changes between 11-14MPa.

Described rectifying column is the stainless steel helices rectifying column.

The temperature of described separative element is 40-45 ℃, and pressure is 6-6.5MPa, extracts preceding 4 hours, and when rectifying column pressure was 11MPa, isolated refine fish oil was rich in EPA, EPA＞43% wherein, DHA＜28%; Back 4 hours when rectifying column pressure is 14MPa, obtains being rich in the refine fish oil of DHA; DHA＞64% wherein, EPA＜10%, the total recovery of EPA+DHA is up to 90%.

Described supercritical CO ₂Separator, the cyclone separator that similar is general, the extraction mixture behind the cooling decompression tangentially enters described separator, separates back CO ₂Discharge from its top, extract fish oil is discharged from its bottom.

Further detailed explanation of the present invention reaches embodiment in conjunction with the accompanying drawings and is described as follows:

Fig. 1 is two liter extracting rectifying segregation apparatus flow charts.

Fig. 2 is 300 liter extracting rectifying segregation apparatus flow charts.

As shown in the figure, 1 is CO ₂Pump, 2 is the raw material dosing pump, and 3 for giving hot device, and 4 is extraction kettle, and 5 is four sections rectifying columns, and 6 is the separator I, and 7 is the separator II, and 8 is CO ₂Depurator, 9 is condenser, 10 is CO ₂Gas cylinder.

As shown in Figure 1, the rough fish oil ethyl ester raw material of raw material adds extraction kettles 4 through measuring pump 2, stop valve 13, reach specified temperature and pressure after, open CO₂Pump 1, CO₂From CO₂Tank 10, condenser 9 through pump 1, give hot device 3 and enter from extraction kettle 4 bottoms, after reaching rated pressure and temperature, enter from the bottom of four sections rectifying columns 5, compress into capable rectifying with control each section column temperature and post from bottom to top, the product that comes out from rectifying column 5 tops, enter separator 6, in case of necessity again through separator 7, CO₂From dividing Discharge from the device top, recycle through clarifier 8 retrieval systems. The rectifying products obtained therefrom is from separator 6 Or 7 bottom emits.

As shown in Figure 2, raw material injects extractors 4 through pump 2, transfer to rated temperature after, by CO₂Pump 1 enters extraction kettle 4 after hot device 3, reach rated temperature and pressure after, enter through the bottom from rectifying column 4, the column temperature of each section and post are pressed from bottom to top, carry out rectifying, from the product that comes out through smart column top, through three grades of cyclonic separation, CO₂Discharge from the separator top, the retrieval system circulation makes behind clarifier 8 With; Product fish oil is discharged in the separator bottom.

The apparent advantage of the present invention is as follows:

1. the content height of fish oil soft capsule DHA of the present invention and EPA, ratio is high and adjustable, because of And functional health is effective, different crowd, is that different purposes (such as brain tonic or the strong heart etc.) are edible different The DHA of ratio and EPA are in order to obtain best effect.

2．CO ₂As extractant, noresidue in the product.

Embodiments of the invention are as follows:

Embodiment 1

Adopt flow process shown in Figure 1.Get rough fish oil 400 grams, EPA+DHA＜30% by step recited above, injects extraction kettle 4 with pump 2, injects CO with pump 1 ₂, at 34 ℃ of temperature, pressure 11.0MPa, CO ₂Extract under the flow 14Kg/H, enter four sections rectifying columns then, from bottom to top, 37 ℃ of 1 section column temperatures, 42 ℃ of 2 sections column temperatures, 47 ℃ of 3 sections column temperatures, 52 ℃ of 4 sections column temperatures carry out rectification under the rectifying column 5 outlet pressure 12MPa, after the decompression cooling, the pressure of separator 6 is transferred to 6MPa, when temperature transfers to 40 ℃, with this understanding, 4 hours inner separator 6 bottoms obtain being rich in the fish oil of EPA, wherein, EPA＞43%, DHA＜28%, behind the extracting rectifying 4 hours, post is pressed and is carried to 14.0MPa, obtains being rich in the fish oil of DHA from separator 7 bottoms, wherein DHA＞64%, EPA＜10%, be rich in EPA product 250 grams, be rich in DHA fish oil product 90 grams, total recovery is up to 85%.

Embodiment 2

Adopt the described flow process of Fig. 1.Rough fish oil ethyl ester 400 grams, EPA+DHA＜30%, 38 ℃ of extraction temperature, pressure 14.0MPa, CO ₂Flow 18Kg/H, 1 section 39 ℃ of rectifying column column temperatures, 2 sections 44 ℃, 3 sections 49 ℃, 4 sections 54 ℃, column outlet pressure 11.0MPa, decompression is cooled to 6.5MPa, 40 ℃, must be rich in EPA fish oil product in preceding 4 hours, EPA＞43% wherein, DHA＜28% extracts after 4 hours, carry behind the post to 14.0MPa, other are the same, obtain being rich in the product of DHA, DHA＞64%, EPA＜10% is rich in EPA product 270 grams, be rich in DHA product 95 grams, total recovery is up to 91%, and all the other are with embodiment 1.

Embodiment 3

Adopt the described production procedure of Fig. 2.100 kilograms of feed purification fish oil ethyl esters, 34 ℃ of extraction temperature, pressure 11.0MPa, CO ₂Flow 1400Kg/H; The rectification column temperature: 1 section 37 ℃, 2 sections 42 ℃, 3 sections 48 ℃, 4 sections 52 ℃, rectification pressure 12.5MPa; 40 ℃ of separator temperatures, pressure 6.5MPa must be rich in the EPA product in preceding 5 hours, EPA＞43% wherein, DHA＜28% must be rich in DHA product 22.5kg in back 5 hours, DHA＞64% wherein, EPA＜10%, total recovery 85%, all the other are with embodiment 1.

Claims

1. high concentration fish oil soft capsule is made of soft capsule parcel fish oil, it is characterized in that DHA and EPA content are 71-74% in the described fish oil, DHA/EPA=3-5.

2. the supercritical CO of concentrated fish oil as claimed in claim 1 ₂The method for making of extracting rectifying comprises the supercritical CO of rough fish oil ₂The reception of extraction, separation, products of separated and CO ₂Circulation, it is characterized in that described raw material is a fish oil ethyl ester, described extraction with separate between set up extract at supercritical CO ₂Rectification under the state separates, and the pressure of described extraction is 11-14MPa, temperature 34-38 ℃; Described rectification pressure is 11-14MPa, and 1 section column temperature 37-39 ℃, 2 sections column temperature 42-44 ℃, 3 sections column temperature 47-49 ℃, 4 sections column temperature 52-54 ℃, described separating pressure is 6.0-6.5MPa, temperature 40-45 ℃, control isolating pressure and temperature, and can obtain different product.